CN106745333A - 黄钠铁矾渣制备镍锌铁氧体的方法 - Google Patents
黄钠铁矾渣制备镍锌铁氧体的方法 Download PDFInfo
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- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 23
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims 8
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 title claims 8
- 229910000359 iron(II) sulfate Inorganic materials 0.000 title claims 8
- 229910052708 sodium Inorganic materials 0.000 title claims 8
- 239000011734 sodium Substances 0.000 title claims 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000706 filtrate Substances 0.000 claims abstract description 17
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000011701 zinc Substances 0.000 claims abstract description 8
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 7
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 6
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 230000001376 precipitating effect Effects 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 1
- 239000013049 sediment Substances 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 229910052935 jarosite Inorganic materials 0.000 abstract description 13
- 239000002893 slag Substances 0.000 abstract description 13
- 239000002244 precipitate Substances 0.000 abstract description 11
- 238000000975 co-precipitation Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 6
- 239000012153 distilled water Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 8
- 238000010979 pH adjustment Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910001035 Soft ferrite Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- KOMIMHZRQFFCOR-UHFFFAOYSA-N [Ni].[Cu].[Zn] Chemical compound [Ni].[Cu].[Zn] KOMIMHZRQFFCOR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- SVKYAACJXKSYTO-UHFFFAOYSA-N iron;nickel;oxozinc Chemical compound [Ni].[Zn].[Fe]=O SVKYAACJXKSYTO-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/80—Compounds containing nickel, with or without oxygen or hydrogen, and containing one or more other elements
- C01G53/82—Compounds containing nickel, with or without oxygen or hydrogen, and containing two or more other elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Soft Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
- Magnetic Ceramics (AREA)
Abstract
本发明涉及一种黄钠铁矾渣制备镍锌铁氧体的方法。黄钠铁矾渣制备镍锌铁氧体的方法，包括如下步骤：称取1g干燥后的黄钠铁矾渣，按Ni0.5Zn0.5Fe2O4计量补加硫酸锌、硫酸镍，加入硫酸溶液水浴搅拌溶解，过滤；用正丁胺将滤液调节pH值至10～11，搅拌反应30 min，陈化1 h；抽滤，用蒸馏水洗沉淀物至无氨味，将沉淀物于80℃下烘干，焙烧2h，冷却，得镍锌铁氧体。本发明以以正丁胺为沉淀剂，黄钠铁矾渣为原料，在室温条件下，通过化学共沉淀法制备得到镍锌铁氧体，具有良好的磁性能。
Description
技术领域
本发明涉及一种黄钠铁矾渣制备镍锌铁氧体的方法。
背景技术
镍锌铁氧体具有高频、宽频、高阻抗、低损耗等特点，成为在高频范围(1～100MHz)内性能优异、应用最广的软磁铁氧体材料，近年越来越受到重视。
目前，国内外报道有关镍锌铁氧体的制备方法主要有高温煅烧法、自蔓延高温合成法、低热固相化学反应法、水热法、化学共沉淀法和溶胶一凝胶法等。其中化学共沉淀法因其工艺简单、产品纯度高、反应温度低、颗粒均匀且粒径小等优点得到格外重视。通过对化学共沉淀法制备镍-铜-锌铁氧体前驱体的热力学行为进行了研究，表明，在Me-NaOH-H2O体系中，当pH值=10～11时，各金属离子可完全共沉淀；在Me-NH4HCO3 -H2O体系中，由于NH3与Zn2+、Ni2+、Cu2+这3种离子络合能力很强，很难使各金属离子共沉淀。所以，在化学共沉淀法中，以正丁胺为共沉淀剂，不仅可以避免引入杂质钠离子，而且可以避免因氨与锌形成可溶性配合物而不参与共沉淀。另外，过滤后滤液中的正丁胺亦可通过蒸馏回收再利用。
发明内容
本发明旨在提出一种黄钠铁矾渣制备镍锌铁氧体的方法。
本发明的技术方案在于：
黄钠铁矾渣制备镍锌铁氧体的方法，包括如下步骤：
称取1~1.5g干燥后的黄钠铁矾渣，按Ni0.5Zn0.5Fe2O4计量加入硫酸锌、硫酸镍，加入硫酸溶液水浴搅拌溶解，过滤；
将滤液调节pH值至10～11，搅拌反应30~40 min，陈化1~1.2 h；抽滤，用蒸馏水洗沉淀物至无氨味，将沉淀物于80~85℃下烘干，焙烧1.5~2h，冷却，得镍锌铁氧体。
所述的硫酸溶液的体积为80~100 mL ，浓度为1~1.5 moL／L。
所述的水浴温度为80~90℃，水浴时间为48~52min。
所述的焙烧温度为70~85℃，焙烧时间为8~10min。
所述的调节滤液pH值通过添加正丁胺实现。
所述的用正丁胺将滤液调节pH值至10.5。
本发明的技术效果在于：
本发明以以正丁胺为沉淀剂，黄钠铁矾渣为原料，在室温条件下，通过化学共沉淀法制备得到镍锌铁氧体，具有良好的磁性能。相比于水热法制备出的镍锌铁氧体，具有更低的比剩余磁化强度和低矫顽力。样品也符合典型的软磁材料低比剩余磁化强度和低矫顽力的特征，应用更广泛。
具体实施方式
黄钠铁矾渣制备镍锌铁氧体的方法，包括如下步骤：
实施例1
称取1g干燥后的黄钠铁矾渣，按Ni0.5Zn0.5Fe2O4计量加入硫酸锌、硫酸镍，加入硫酸溶液水浴搅拌溶解，过滤；
将滤液调节pH值至10，搅拌反应30 min，陈化1 h；抽滤，用蒸馏水洗沉淀物至无氨味，将沉淀物于80℃下烘干，焙烧1.5h，冷却，得镍锌铁氧体。
其中，所述的硫酸溶液的体积为80 mL ，浓度为1 moL／L。所述的水浴温度为80℃，水浴时间为48min。所述的焙烧温度为70℃，焙烧时间为8min。所述的调节滤液pH值通过添加正丁胺实现。所述的用正丁胺将滤液调节pH值至10.5。
实施例2
称取1.5g干燥后的黄钠铁矾渣，按Ni0.5Zn0.5Fe2O4计量加入硫酸锌、硫酸镍，加入硫酸溶液水浴搅拌溶解，过滤；
将滤液调节pH值至111，搅拌反应40 min，陈化1.2 h；抽滤，用蒸馏水洗沉淀物至无氨味，将沉淀物于85℃下烘干，焙烧2h，冷却，得镍锌铁氧体。
其中，所述的硫酸溶液的体积为100 mL ，浓度为1.5 moL／L。所述的水浴温度为90℃，水浴时间为52min。所述的焙烧温度为85℃，焙烧时间为10min。所述的调节滤液pH值通过添加正丁胺实现。所述的用正丁胺将滤液调节pH值至10.5。
实施例3
称取1.2g干燥后的黄钠铁矾渣，按Ni0.5Zn0.5Fe2O4计量加入硫酸锌、硫酸镍，加入硫酸溶液水浴搅拌溶解，过滤；
将滤液调节pH值至10，搅拌反应35 min，陈化1 h；抽滤，用蒸馏水洗沉淀物至无氨味，将沉淀物于82℃下烘干，焙烧1.8h，冷却，得镍锌铁氧体。
其中，所述的硫酸溶液的体积为90 mL ，浓度为1.2moL／L。所述的水浴温度为85℃，水浴时间为50min。所述的焙烧温度为80℃，焙烧时间为9min。所述的调节滤液pH值通过添加正丁胺实现。所述的用正丁胺将滤液调节pH值至10.5。
Claims (6)
1.黄钠铁矾渣制备镍锌铁氧体的方法，其特征在于：包括如下步骤：
称取1~1.5g干燥后的黄钠铁矾渣，按Ni0.5Zn0.5Fe2O4计量加入硫酸锌、硫酸镍，加入硫酸溶液水浴搅拌溶解，过滤；
将滤液调节pH值至10～11，搅拌反应30~40 min，陈化1~1.2 h；抽滤，用蒸馏水洗沉淀物至无氨味，将沉淀物于80~85℃下烘干，焙烧1.5~2h，冷却，得镍锌铁氧体。
2.根据权利要求1所述的黄钠铁矾渣制备镍锌铁氧体的方法，其特征在于：所述的硫酸溶液的体积为80~100 mL ，浓度为1~1.5 moL／L。
3.根据权利要求1所述的黄钠铁矾渣制备镍锌铁氧体的方法，其特征在于：所述的水浴温度为80~90℃，水浴时间为48~52min。
4.根据权利要求1所述的黄钠铁矾渣制备镍锌铁氧体的方法，其特征在于：所述的焙烧温度为70~85℃，焙烧时间为8~10min。
5.根据权利要求1所述的黄钠铁矾渣制备镍锌铁氧体的方法，其特征在于：所述的调节滤液pH值通过添加正丁胺实现。
6.根据权利要求1所述的黄钠铁矾渣制备镍锌铁氧体的方法，其特征在于：所述的用正丁胺将滤液调节pH值至10.5。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109192434A (zh) * | 2018-09-21 | 2019-01-11 | 佛山皖和新能源科技有限公司 | 一种软磁铁氧体材料的制备方法 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109192434A (zh) * | 2018-09-21 | 2019-01-11 | 佛山皖和新能源科技有限公司 | 一种软磁铁氧体材料的制备方法 |
| CN109192434B (zh) * | 2018-09-21 | 2020-08-21 | 江门杰富意磁性材有限公司 | 一种软磁铁氧体材料的制备方法 |
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